Water → 2,3-Dichloro-6-(trifluoromethyl)benzonitrile

HRID 1005482노트

반응식

HRID 1005482 반응식
[Cl:1][C:2]1[C:10]([Cl:11])=[CH:9][CH:8]=[C:7]([C:12]([F:15])([F:14])[F:13])[C:3]=1[C:4]([NH2:6])=O.P(Cl)(Cl)(Cl)=O.O>C1C=CC=CC=1>[Cl:1][C:2]1[C:10]([Cl:11])=[CH:9][CH:8]=[C:7]([C:12]([F:15])([F:13])[F:14])[C:3]=1[C:4]#[N:6]

참가 물질

5

반응물 3

HCID 962WaterHCID 24813Phosphorus oxychloride2회HCID 154569832,3-Dichloro-6-(trifluoromethyl)benzamide

생성물 1

HCID 109775462,3-Dichloro-6-(trifluoromethyl)benzonitrile수율 95.8%

시약·촉매·용매 1

HCID 241Benzene용매

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온도
35 °C

실험 절차

To a solution of 229 g of 2,3-dichloro-6-trifluoromethylbenzamide in 2 liters of benzene was added 409 g of phosphorus oxychloride and then the mixture was heated at ref lux for 3.5 hours. After cooling, the solution was gradually added into 2 liters of water maintained at 30-40° C. to hydrolyze the excess phosphorus oxychloride therein and was allowed to separation. The aqueous layer was extracted with benzene, and the extract was combined with the organic layer previously obtained, washed with water and with saturated saline solution and dried over anhydrous magnesium sulfate. The solvent was distilled under reduced pressure, and the crude product obtained was washed with n-hexane and filtered to obtain 204 g of the title compound(mp. 53-54° C.).

후처리

  1. temperaturethe mixture was heated at ref lux for 3.5 hours
  2. temperatureAfter cooling
  3. customwas allowed to separation
  4. extractionThe aqueous layer was extracted with benzene
  5. custompreviously obtained
  6. washwashed with water and with saturated saline solution
  7. dry with materialdried over anhydrous magnesium sulfate
  8. distillationThe solvent was distilled under reduced pressure
  9. customthe crude product obtained
  10. washwas washed with n-hexane
  11. filtrationfiltered

출처 및 근거

ORD 기록
ord-bf5c0b36694746b98409c37ab334a751
출처 데이터셋
uspto-grants-2000_04
특허 번호
US06054605

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